CN111218664A - Microwave-based artificial diamond preparation process - Google Patents
Microwave-based artificial diamond preparation process Download PDFInfo
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- CN111218664A CN111218664A CN202010163402.9A CN202010163402A CN111218664A CN 111218664 A CN111218664 A CN 111218664A CN 202010163402 A CN202010163402 A CN 202010163402A CN 111218664 A CN111218664 A CN 111218664A
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- Prior art keywords
- diamond
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- cvd
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/277—Diamond only using other elements in the gas phase besides carbon and hydrogen; using other elements besides carbon, hydrogen and oxygen in case of use of combustion torches; using other elements besides carbon, hydrogen and inert gas in case of use of plasma jets
Abstract
The invention discloses a microwave-based artificial diamond preparation process which is characterized by comprising the following steps of: s1, preprocessing the diamond master slice and drying the diamond master slice for later use; s2, putting the diamond into a CVD diamond growing furnace, and vacuumizing the furnace; s3, introducing mixed gas of CH4 and H2; s4, controlling the pressure in the furnace to be 30-40 KPa; s5: microwave heating, adjusting the surface temperature of the processing cutter to 800-900 ℃, and depositing for 10-12 h to form a diamond coating; s6: introducing N2 into the CVD diamond growing furnace, and gradually increasing the airflow rate of N2 until the airflow rate ratio of CH4, H2 and Ar is 20: 100-300: 5-300. The invention discloses a method for introducing N2 (nitrogen gas) into a CVD diamond growing furnace, which can not only ensure the color and the cleanliness of the original diamond, but also rapidly increase the thickness by dozens of times, save half time compared with the common method, and enable the diamond to grow better and faster.
Description
Technical Field
The invention relates to the technical field of artificial diamond preparation processes, in particular to a microwave-based artificial diamond preparation process.
Background
Diamond is the hardest substance among the known materials, has high thermal conductivity and wear resistance, making it widely used in various superhard cutters, heat sinks, and other fields. In the jewelry field, diamonds are popular with people as souvenirs and are the first choice gifts for marrying and expressing love. However, natural diamonds are very rare and expensive, and the presence of artificial diamonds remedies this disadvantage.
Currently, most of the artificial diamonds are made by high temperature and high pressure process. There are patent reports that bone ash and human hair are used as solid carbon sources, and a high-temperature high-pressure process is adopted to grow diamonds with memorial significance. The process is complex in that the artificial diamond is grown by carbonizing and extracting a solid carbon source and then performing high temperature and high pressure on the solid carbon source. Moreover, bone ash is used as a carbon source, which involves moral problems and is not accepted by people. Moreover, the existing method can not ensure the color and the cleanliness of the artificial diamond and has slower production speed.
Disclosure of Invention
The invention aims to provide a microwave artificial diamond preparation process which can ensure the color and the cleanliness of the original diamond and can rapidly increase the thickness of the original diamond by dozens of times.
In order to achieve the purpose, the invention adopts the following technical scheme:
a microwave-based artificial diamond preparation process comprises the following steps:
s1, preprocessing the diamond master slice and drying the diamond master slice for later use;
s2, putting the diamond into a CVD diamond growing furnace, and vacuumizing the furnace;
s3, introducing mixed gas of CH4 and H2;
s4, controlling the pressure in the furnace to be 30-40 KPa;
s5: microwave heating, adjusting the surface temperature of the processing cutter to 800-900 ℃, and depositing for 10-12 h to form a diamond coating;
s6: introducing N2 into the CVD diamond growing furnace, and gradually increasing the airflow rate of N2 until the airflow rate ratio of CH4, H2 and Ar is 20: 100-300: 5-300.
Preferably, in the step S3, the mixed gas of CH4 and H2 is introduced according to the airflow rate ratio of CH4 to H2 of 20: 100-300.
Preferably, the pressure in the furnace is adjusted to be 30-40 KPa, and the ratio of the gas flow rates of CH4 and H2 is kept unchanged.
Preferably, in the step S6, the pressure in the CVD diamond growth furnace is maintained at 30 to 40KPa, the temperature of the surface of the processing tool is controlled at 800 to 900 ℃, and the reaction time is maintained at 380 to 400 hours.
Preferably, the concentration of N2 is less than 10%.
Preferably, the concentration of N2 is less than 5%.
The invention discloses that N2 (nitrogen gas) is introduced into a CVD diamond growing furnace, which not only can ensure the color and the cleanliness of the original diamond, but also can rapidly increase the thickness by dozens of times, can save half time compared with the prior art, and can ensure that the diamond grows better and faster.
Detailed Description
The invention provides a microwave-based artificial diamond preparation process, which comprises the following steps:
s1, preprocessing the diamond master slice and drying the diamond master slice for later use;
s2, putting the diamond into a CVD diamond growing furnace, and vacuumizing the furnace;
s3, introducing mixed gas of CH4 and H2 according to the airflow rate ratio of CH4 to H2 of 20: 100-300;
s4, controlling the pressure in the furnace to be 30-40 KPa;
s5: microwave heating, adjusting the surface temperature of the processing cutter to 800-900 ℃, and depositing for 10-12 h to form a diamond coating;
s6: and adjusting the pressure in the furnace to be 30-40 KPa, and keeping the ratio of the CH4 airflow rate to the H2 airflow rate unchanged.
S7: introducing N2 into the CVD diamond growth furnace, gradually increasing the airflow rate of N2 until the airflow rate ratio of CH4, H2 and Ar is 20: 100-300: 5-300, maintaining the pressure in the CVD diamond growth furnace at 30-40 KPa, controlling the temperature of the surface of the processing cutter at 800-900 ℃, and maintaining the reaction time for 380-400H.
The results of multiple experiments prove that when the concentration of N2 (nitrogen) is lower than 5%, the growth rate of the diamond is greatly improved, and the growth quality is good.
When the nitrogen concentration exceeds 10%, the diamond growth rate gradually approaches saturation, the non-diamond phase is continuously increased, and the growth quality is continuously reduced.
The invention discloses that N2 (nitrogen gas) is introduced into a CVD diamond growing furnace, which not only can ensure the color and the cleanliness of the original diamond, but also can rapidly increase the thickness by dozens of times, can save half time compared with the prior art, and can ensure that the diamond grows better and faster.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention should be covered by the scope of the present invention.
Claims (6)
1. A microwave-based artificial diamond preparation process is characterized by comprising the following steps:
s1, preprocessing the diamond master slice and drying the diamond master slice for later use;
s2, putting the diamond into a CVD diamond growing furnace, and vacuumizing the furnace;
s3, introducing mixed gas of CH4 and H2;
s4, controlling the pressure in the furnace to be 30-40 KPa;
s5: microwave heating, adjusting the surface temperature of the processing cutter to 800-900 ℃, and depositing for 10-12 h to form a diamond coating;
s6: introducing N2 into the CVD diamond growing furnace, and gradually increasing the airflow rate of N2 until the airflow rate ratio of CH4, H2 and Ar is 20: 100-300: 5-300.
2. The process of claim 1, wherein in step S3, the gas mixture of CH4 and H2 is introduced at a ratio of CH4 to H2 to 20: 100-300.
3. The process of claim 2, wherein the pressure in the furnace is adjusted to 30 to 40KPa, and the gas flow rate ratio of CH4 to H2 is kept constant.
4. The process of claim 1, wherein the pressure in the CVD Diamond growth furnace is maintained at 30-40 KPa, the temperature of the surface of the processing tool is controlled at 800-900 ℃, and the reaction time is maintained at 380-400 h.
5. A process for preparing artificial diamond according to claim 1, wherein the concentration of N2 is less than 10%.
6. A process for preparing artificial diamond according to claim 1, wherein the concentration of N2 is less than 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010163402.9A CN111218664A (en) | 2020-03-10 | 2020-03-10 | Microwave-based artificial diamond preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010163402.9A CN111218664A (en) | 2020-03-10 | 2020-03-10 | Microwave-based artificial diamond preparation process |
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| CN111218664A true CN111218664A (en) | 2020-06-02 |
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| CN202010163402.9A Pending CN111218664A (en) | 2020-03-10 | 2020-03-10 | Microwave-based artificial diamond preparation process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388886A (en) * | 2021-07-30 | 2021-09-14 | 杨钧夫 | Culture method of commemorative diamond |
Citations (7)
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| CN101311339A (en) * | 2008-04-25 | 2008-11-26 | 吉林大学 | Process for discriminating high growth rate chemical vapour deposition diamond single crystal |
| US20100242834A1 (en) * | 2009-03-31 | 2010-09-30 | Rajneesh Bhandari | Method for producing single crystalline diamonds |
| CN103154331A (en) * | 2010-09-27 | 2013-06-12 | 二A科技有限公司 | Method for growing white color diamonds by using diborane and nitrogen in combination in a microwave plasma chemical vapor deposition system |
| US20150222087A1 (en) * | 2012-08-13 | 2015-08-06 | Element Six Technologies Limited | Thick polycrystalline synthetic diamond wafers for heat spreading applications and microwave plasma chemical vapour depositon synthesis techniques |
| CN106222628A (en) * | 2016-08-31 | 2016-12-14 | 廊坊西波尔钻石技术有限公司 | The preparation method of a kind of Jubilee and device |
| CN108315716A (en) * | 2018-02-07 | 2018-07-24 | 上海三朗纳米技术有限公司 | A kind of composite coating preparation process based on process tool |
| CN109295434A (en) * | 2018-11-27 | 2019-02-01 | 江苏沃德赛模具科技有限公司 | Micropore surface nano-diamond coating |
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2020
- 2020-03-10 CN CN202010163402.9A patent/CN111218664A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311339A (en) * | 2008-04-25 | 2008-11-26 | 吉林大学 | Process for discriminating high growth rate chemical vapour deposition diamond single crystal |
| US20100242834A1 (en) * | 2009-03-31 | 2010-09-30 | Rajneesh Bhandari | Method for producing single crystalline diamonds |
| CN103154331A (en) * | 2010-09-27 | 2013-06-12 | 二A科技有限公司 | Method for growing white color diamonds by using diborane and nitrogen in combination in a microwave plasma chemical vapor deposition system |
| US20150222087A1 (en) * | 2012-08-13 | 2015-08-06 | Element Six Technologies Limited | Thick polycrystalline synthetic diamond wafers for heat spreading applications and microwave plasma chemical vapour depositon synthesis techniques |
| CN106222628A (en) * | 2016-08-31 | 2016-12-14 | 廊坊西波尔钻石技术有限公司 | The preparation method of a kind of Jubilee and device |
| CN108315716A (en) * | 2018-02-07 | 2018-07-24 | 上海三朗纳米技术有限公司 | A kind of composite coating preparation process based on process tool |
| CN109295434A (en) * | 2018-11-27 | 2019-02-01 | 江苏沃德赛模具科技有限公司 | Micropore surface nano-diamond coating |
Non-Patent Citations (1)
| Title |
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| 夏禹豪等: ""MPCVD 法中氮气对单晶金刚石生长机理影响的探究"", 《真空科学与技术学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388886A (en) * | 2021-07-30 | 2021-09-14 | 杨钧夫 | Culture method of commemorative diamond |
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